CN115501689B - Method for continuously classifying and collecting micron-sized particles dispersed in slurry - Google Patents

Method for continuously classifying and collecting micron-sized particles dispersed in slurry Download PDF

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CN115501689B
CN115501689B CN202211150799.3A CN202211150799A CN115501689B CN 115501689 B CN115501689 B CN 115501689B CN 202211150799 A CN202211150799 A CN 202211150799A CN 115501689 B CN115501689 B CN 115501689B
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particles
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micron
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CN115501689A (en
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陈秋飞
郭鹏宗
张贺平
孟强
郑皓宇
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Zhongfu Shenying Carbon Fiber Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D36/00Filter circuits or combinations of filters with other separating devices
    • B01D36/04Combinations of filters with settling tanks
    • B01D36/045Combination of filters with centrifugal separation devices

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Abstract

The invention discloses a method for continuously classifying and collecting micron-sized particles dispersed in slurry. The method comprises the steps of screening micron-sized particles in slurry layer by layer in three stages, fully mashing and washing wet materials in the centrifuging process, adding hot water, centrifuging at high speed twice, fully drying the wet materials, and crushing to obtain first-third-stage micron-sized particle products. The method can realize continuous three-stage screening and collection of the micron-sized particle products, and effectively collect the micron-sized particle products with volume average particle diameters of 4-6 mu m, 10-13 mu m and 25-32 mu m.

Description

Method for continuously classifying and collecting micron-sized particles dispersed in slurry
Technical Field
The invention belongs to the technical field of particle classification, and relates to a method for continuously classifying and collecting micron-sized particles dispersed in slurry.
Background
The slurry material in the chemical production process is mixed slurry composed of micron-sized particles, water, a small amount of organic solvent and the like. In the processes of wet sieving, centrifuging, washing, filtering and the like, the slurry has micron-sized particle products and non-product components separated, micron-sized particles are subjected to grading (separation) treatment and limited-size particles are subjected to classified collection, and specific requirements are provided for the design, the functionality and the chemical production process of chemical equipment. Based on the material characteristics of micron-sized particles and the diversity requirements of the limited sizes of products, various separation equipment, separation and collection methods are invented, the chemical production efficiency is improved, the purpose of classifying and collecting the limited sizes of micron-sized particle products is also realized, and the method plays a substantial promotion role in the development of the chemical industry. The unit operations play an important role in chemical production, and are widely applied to the industrial fields of materials, medicines and the like which have common characteristics with chemical industry.
The existing chemical production has the problems that the size span of the particles which are classified and collected is large, the normal distribution range of the particle sizes is large, and the stability of the product performance is low for the micron-sized particles, and aiming at the classification screening and classification collection of micron-sized particle products, no complete technological treatment process, classification and collection method exists, so that hidden danger is brought to the production of downstream composite materials of micron-sized particle materials and the stability of the product performance, and the product quality is difficult to effectively guarantee.
Disclosure of Invention
The invention aims to provide a method for continuously classifying and collecting micron-sized particles dispersed in slurry.
The technical scheme for realizing the purpose of the invention is as follows:
the continuous classifying and collecting process of micron level grains dispersed in slurry includes the steps of solid-liquid separation of slurry in electric vibrating screen and centrifugal filter cloth, flushing with hot water at 70-80 deg.c to obtain three kinds of micron level grains in different sizes, and the steps of:
(1) Passing the slurry through a first-stage electric vibration screen to remove large-size particles with the particle size larger than 38.5 mu m, adding a small amount of hot water with the temperature of 70-80 ℃ for flushing in the sieving process, enhancing the sieving effect, temporarily storing the slurry passing through the screen in a heat insulation device, and counting the volume of the slurry to be V 1
(2) Adding the slurry obtained in the step (1) through a screen into a first-stage filter bag, and centrifuging at a high speed of 1500-2000 r/min to remove particles and filtrate with particle diameters smaller than 22 mu m, wherein hot water with the temperature of 70-80 ℃ is added in batches during the process, and the total amount of the added hot water is 8-10V 1 Centrifuging twice, wherein the adding amount of hot water is 4-5V each time 1 The method comprises the steps of carrying out a first treatment on the surface of the After the first centrifugation, mashing and washing the solid wet material, adding hot water again for high-speed centrifugation for 30-40 min until no filtrate flows out, and then carrying out the next step;
(3) Collecting the particles in the step (2) which are retained in the first-stage filter bag, and fully drying to obtain first-stage micron-sized particles with volume average particle size of 25-32 mu m;
(4) Collecting the slurry passing through the filter cloth in the step (2), and then passing through a second-stage electric vibration screen to remove large-size particles with the particle size larger than 15 mu m, wherein the slurry passing through the screen is temporarily stored in heat insulation equipment, and the volume of the slurry is calculated to be V 2
(5) Adding the slurry obtained in the step (4) into a second-stage filter bag, and performing high-speed centrifugation at 1500-2000 r/min to remove particles with particle size smaller than 8 μm and filtrate, wherein hot water with the temperature of 70-80 ℃ is added in batches during the process, and the total amount of the added hot water is 2-4V 2 Centrifuging twice, wherein the hot water quantity added each time is 1-2V 2 The method comprises the steps of carrying out a first treatment on the surface of the After the first centrifugation, mashing and washing the solid wet material, adding hot water again for high-speed centrifugation for 30-40 min until no filtrate flows out, and then carrying out the next step;
(6) Collecting the particles remained in the second-stage filter bag in the step (5), and fully drying to obtain second-stage micron-sized particles with volume average particle diameter of 10-13 μm;
(7) Adding all the slurry in the step (5) into a third-stage filter bag, and performing high-speed centrifugation at 1500-2000 r/min to remove particles and filtrate with particle diameters smaller than 3 mu m until no filtrate flows out, and performing the next step;
(8) And (3) collecting the particles remained in the third-stage filter bag in the step (7), and fully drying to obtain the third-stage micron-sized particles with the volume average particle size of 4-6 mu m.
The micron-sized particles are composite toughening particles formed by reacting a polymer, epoxy resin and a curing agent, are commonly used in carbon fiber composite reinforced materials, and have a core-shell structure, wherein the core in the core-shell structure is composed of the polymer, and the three-dimensional network structure formed by reacting the epoxy resin and the curing agent is composed of the shell in the core-shell structure. Such polymers include, but are not limited to, polyethersulfones, polyurethanes, polyamides, polyimides, polycarbonates, and the like.
Preferably, in the step (1), the first-stage electric vibration screen is made of 316L material, the mesh number is 400, and the screen pore diameter is 38.5 μm.
Preferably, in the step (2), the first stage filter bag is made of polypropylene, the mesh number is 800, and the pore diameter of the filter screen is 22 μm.
Preferably, in the step (3), the second-stage electric vibration screen is made of 316L material, the mesh number is 1000 meshes, and the screen pore diameter is 15 μm.
Preferably, in the step (4), the second-stage filter bag is made of polypropylene, the mesh number is 2000 mesh, and the pore diameter of the filter screen is 8 mu m.
Preferably, in the step (7), the third stage filter bag is made of polypropylene, the mesh number is 2800 mesh, and the pore diameter of the filter screen is 3 μm.
The method comprises the steps of screening micron-sized particles layer by layer in three stages, fully mashing and washing wet materials in the centrifugation process, adding hot water, carrying out high-speed centrifugation twice, fully drying and crushing the wet materials to obtain first-third-stage micron-sized particle products. The method can realize continuous three-stage screening and collection of the micron-sized particle products, and effectively collect the micron-sized particle products with volume average particle diameters of 4-6 mu m, 10-13 mu m and 25-32 mu m.
Drawings
FIG. 1 is a schematic flow chart of a method for continuously classifying and collecting micron-sized particles dispersed in a slurry according to the present invention.
Detailed Description
The invention will be further elucidated with reference to the drawings and to specific embodiments.
In the invention, the micron-sized particles are composite toughening particles formed by reacting a polymer, epoxy resin and a curing agent, are commonly used in carbon fiber composite reinforced materials, and have a core-shell structure, wherein the core in the core-shell structure is composed of the polymer, and the three-dimensional network structure formed by reacting the epoxy resin and the curing agent forms a shell in the core-shell structure. Such polymers include, but are not limited to, polyethersulfones, polyurethanes, polyamides, polyimides, polycarbonates, and the like, such as disclosed in chinese patent No. 103717653B as ultrafine particles formed by compounding an epoxy resin, an epoxy resin curing agent, and polymer particles insoluble in the epoxy resin.
Example 1
(1) Firstly, passing 20L of slurry through a first-stage electric vibration screen (316L material, 400 meshes and screen aperture of 38.5 um), adding 3L of 80 ℃ hot water to wash the first-stage electric vibration screen, temporarily storing the slurry passing through the screen in heat insulation equipment, and measuring the volume of the slurry to be 22.8L;
(2) Adding 22.8L of the slurry obtained in the step (1) into a first-stage filter bag (made of polypropylene material, 800 meshes and having a filter screen aperture of 22 um), and performing high-speed centrifugation (the centrifugal speed is 1800 r/min); 220L of 80 ℃ hot water is added, and the mixture is added in two times, 110L each time; after the first centrifugation, carrying out operations such as mashing, water washing and the like on the solid wet material, adding hot water, carrying out high-speed centrifugation again for 40min, and carrying out the next step after basically no filtrate flows out;
(3) Collecting the particles remained in the first-stage filter bag in the step (2), fully drying to obtain the product which is first-stage micron-sized particles, and sealing and storing at normal temperature;
(4) Collecting the slurry passing through the filter cloth in the step (2), temporarily storing the slurry in heat preservation equipment, passing through a second-stage electric vibration screen (316L material, 1000 meshes and screen aperture 15 um), adding 10L hot water to wash the second-stage electric vibration screen, temporarily storing the slurry passing through the screen in the heat preservation equipment, and measuring the volume of the slurry to be about 249L;
(5) Adding 249L of the slurry in the step (4) into a second-stage filter bag (made of polypropylene, 2000 meshes and provided with a filter screen aperture of 8 um), performing high-speed centrifugation (the rotating speed is 1800 r/min), adding 80 ℃ hot water for 500L in two times, and performing centrifugation operation (the adding amount of hot water is about 250L each time) in two times; after the first centrifugation, the solid wet material is subjected to operations such as mashing, water washing and the like, a second batch of hot water is added for high-speed centrifugation (the rotating speed is 1800 r/min) again for 40min, and the next step can be carried out after no filtrate basically flows out;
(6) Collecting the particles retained in the second-stage filter bag in the step (5), and fully drying to obtain a second-stage micron-sized particle product, and sealing and storing at normal temperature;
(7) Adding all the slurry in the step (5) into a third-stage filter bag (made of polypropylene material and 2800 meshes and provided with a filter screen aperture of 3 um), performing high-speed centrifugation (the centrifugal speed is 2000 r/min), and performing the next step after no filtrate basically flows out;
(8) Collecting the particles retained in the third-stage filter bag in the step (7), and fully drying to obtain a third-stage micron-sized particle product, and sealing and preserving at normal temperature;
(9) The first to third-stage micron-sized particles obtained in the above steps were each obtained by taking 20g of a sample, sufficiently pulverizing the sample by a micro pulverizer, and then performing particle size analysis by using a Microtrac S3500 laser particle size analyzer, thereby obtaining volume average particle diameters of the particles, and the particle size analysis results are shown in table 1.
Table 1 results of particle size analysis of test samples
Comparative example 1
In this comparative example, each stage of product was not washed with water, and the specific steps were as follows:
(1) Passing 20L of slurry through a first-stage electric vibration screen (316L material, 400 meshes and screen aperture of 38.5 um), temporarily storing the slurry passing through the screen in a heat insulation device, and measuring the volume of the slurry to be 17.8L;
(2) Adding 17.8L of the slurry obtained in the step (1) into a first-stage filter bag (made of polypropylene material, 800 meshes and provided with a filter screen aperture of 22 um), performing high-speed centrifugation (the centrifugal speed is 1800 r/min), and performing the next step after no filtrate basically flows out;
(3) Collecting the particles remained in the first-stage filter bag in the step (2), fully drying to obtain the product which is first-stage micron-sized particles, and sealing and storing at normal temperature;
(4) Collecting the slurry passing through the filter cloth in the step (2), temporarily storing the slurry in heat preservation equipment, passing through a second-stage electric vibration screen (316L material, 1000 meshes and screen aperture 15 um), temporarily storing the slurry passing through the screen in the heat preservation equipment, and measuring the volume of the slurry to be about 16.9L;
(5) Adding 16.9L of the slurry obtained in the step (4) into a second-stage filter bag (made of polypropylene material, 2000 meshes and provided with a filter screen aperture of 8 um), performing high-speed centrifugation (with the rotating speed of 1800 r/min), and performing the next step after no filtrate basically flows out;
(6) Collecting the particles retained in the second-stage filter bag in the step (5), and fully drying to obtain a second-stage micron-sized particle product, and sealing and storing at normal temperature;
(7) Adding all the slurry in the step (5) into a third-stage filter bag (made of polypropylene material and 2800 meshes and provided with a filter screen aperture of 3 um), performing high-speed centrifugation (the centrifugal speed is 2000 r/min), and performing the next step after no filtrate basically flows out;
(8) And (3) collecting the particles remained in the third-stage filter bag in the step (7), and fully drying to obtain a third-stage micron-sized particle product, and sealing and storing at normal temperature. The yields of the various stages of products are shown in Table 2.
TABLE 2 yield test results
According to analysis and comparison, the yield of each stage of product without water washing is lower, and the sum of the yields of each stage of product is lower than that of the experimental batch subjected to water washing; the reason is that in the process of passing through the screen, the aperture of the screen is blocked, so that the passing efficiency of the product is reduced, and the yield is reduced. The hot water washing step is necessary for the yield assurance of the product.
Comparative example 2
In the comparative example, each stage of products is washed by water at 30 ℃, and the specific steps are as follows:
(1) Firstly, passing 20L of slurry through a first-stage electric vibration screen (316L material, 400 meshes and screen aperture of 38.5 um), adding 3L of 30 ℃ flushing water to flush the first-stage electric vibration screen, temporarily storing the slurry passing through the screen in heat insulation equipment, and measuring the volume of the slurry to be 22.6L;
(2) Adding 22.6L of the slurry obtained in the step (1) into a first-stage filter bag (made of polypropylene material, 800 meshes and having a filter screen aperture of 22 um), and performing high-speed centrifugation (the centrifugal speed is 1800 r/min); adding 220L of washing water at 30 ℃ into the kettle, wherein the washing water is added in two times of 110L each time; after the first centrifugation, the solid wet material is subjected to operations such as mashing, water washing and the like, washing water at 30 ℃ is added, the high-speed centrifugation is carried out again for 40min, and the next step is carried out after no filtrate basically flows out;
(3) Collecting the particles remained in the first-stage filter bag in the step (2), fully drying to obtain the product which is first-stage micron-sized particles, and sealing and storing at normal temperature;
(4) Collecting the slurry passing through the filter cloth in the step (2), temporarily storing the slurry in heat preservation equipment, passing through a second-stage electric vibration screen (316L material, 1000 meshes and screen aperture 15 um), adding 10L washing water at 30 ℃ to wash the second-stage electric vibration screen, temporarily storing the slurry passing through the screen in the heat preservation equipment, and measuring the volume of the slurry to be about 247L;
(5) Adding 247L of slurry in the step (4) into a second-stage filter bag (made of polypropylene, 2000 meshes and provided with a filter screen aperture of 8 um), performing high-speed centrifugation (the rotating speed is 1800 r/min), adding 500L of washing water at 30 ℃ in two times, and performing centrifugation in two times (the adding amount of washing water is about 250L each time); after the first centrifugation, the solid wet material is subjected to operations such as mashing, water washing and the like, a second batch of washing water at 30 ℃ is added, and the solid wet material is centrifuged at a high speed (the rotating speed is 1800 r/min) for 40min again, so that the next step can be carried out after no filtrate basically flows out;
(6) Collecting the particles retained in the second-stage filter bag in the step (5), and fully drying to obtain a second-stage micron-sized particle product, and sealing and storing at normal temperature;
(7) Adding all the slurry in the step (5) into a third-stage filter bag (made of polypropylene material and 2800 meshes and provided with a filter screen aperture of 3 um), performing high-speed centrifugation (the centrifugal speed is 2000 r/min), and performing the next step after no filtrate basically flows out;
(8) And (3) collecting the particles remained in the third-stage filter bag in the step (7), and fully drying to obtain a third-stage micron-sized particle product, and sealing and storing at normal temperature. The yields of the various stages of products are shown in Table 2.
According to analysis and comparison, the yield of each stage of washing water at 30 ℃ is lower than that of hot water washing, but is slightly higher than that of washing without washing; and the sum of the yields of the products of each stage also shows the same trend. The reason is that in the process of passing through the screen, products at all levels are stored to block the aperture of the screen, and washing water at 30 ℃ cannot effectively open the aperture of the screen, so that the passing efficiency of the products is low, and the yield is low. The 30 c rinse water wash step is not significant in terms of product yield improvement.
Comparative example 3
(1) Firstly, passing 20L of slurry through a first-stage electric vibration screen (316L material, 400 meshes and screen aperture of 38.5 um), adding 1L of 80 ℃ hot water to wash the first-stage electric vibration screen, temporarily storing the slurry passing through the screen in heat insulation equipment, and measuring the volume of the slurry to be 20.6L;
(2) Adding 20.6L of the slurry obtained in the step (1) into a first-stage filter bag (made of polypropylene material, 800 meshes and having a filter screen aperture of 22 um), and performing high-speed centrifugation (the centrifugal speed is 1800 r/min); adding hot water at 80 ℃ for 50L, and adding the hot water in two times, wherein 50L is added each time; after the first centrifugation, carrying out operations such as mashing, water washing and the like on the solid wet material, adding hot water, carrying out high-speed centrifugation again for 40min, and carrying out the next step after basically no filtrate flows out;
(3) Collecting the particles remained in the first-stage filter bag in the step (2), fully drying to obtain the product which is first-stage micron-sized particles, and sealing and storing at normal temperature;
(4) Collecting the slurry passing through the filter cloth in the step (2), temporarily storing the slurry in heat preservation equipment, passing through a second-stage electric vibration screen (316L material, 1000 meshes and screen aperture 15 um), adding 5L hot water to wash the second-stage electric vibration screen, temporarily storing the slurry passing through the screen in the heat preservation equipment, and measuring the volume of the slurry to be about 119.8L;
(5) Adding 119.8L of the slurry obtained in the step (4) into a second-stage filter bag (made of polypropylene, 2000 meshes and provided with a filter screen aperture of 8 um), performing high-speed centrifugation (the rotating speed is 1800 r/min), adding 100L of hot water at 80 ℃ in two times, and performing centrifugation operation in two times (the adding amount of the hot water is about 50L each time); after the first centrifugation, the solid wet material is subjected to operations such as mashing, water washing and the like, a second batch of hot water is added, and the second batch of hot water is subjected to high-speed centrifugation again (the rotating speed is 1800 r/min) for 40min, so that the next step can be carried out after no filtrate basically flows out;
(6) Collecting the particles retained in the second-stage filter bag in the step (5), and fully drying to obtain a second-stage micron-sized particle product, and sealing and storing at normal temperature;
(7) Adding all the slurry in the step (5) into a third-stage filter bag (made of polypropylene material and 2800 meshes and provided with a filter screen aperture of 3 um), performing high-speed centrifugation (the centrifugal speed is 2000 r/min), and performing the next step after no filtrate basically flows out;
(8) And (3) collecting the particles remained in the third-stage filter bag in the step (7), and fully drying to obtain a third-stage micron-sized particle product, and sealing and storing at normal temperature.
TABLE 3 results of sample yield tests with different amounts of flushing water
By analysis and comparison, the yield of each stage of products washed by different washing water amounts is lower than that of the specified hot water amount, and the total yield of each stage of products is also lower. The reason is that in the process of passing through the screen, the aperture of the screen is blocked, and the rinsing water quantity is small enough to ensure that the qualified product passes through the screen, so that the passing efficiency of the product is low and the yield is low. The small amount of hot rinse water wash step is not significant in terms of the yield improvement effect of the product.

Claims (8)

1. A method for continuously classifying and collecting micron-sized particles dispersed in slurry is characterized by comprising the following specific steps:
(1) Passing the slurry through a first-stage electric vibration screen to remove large-size particles with the particle size larger than 38.5 mu m, adding a small amount of hot water with the temperature of 70-80 ℃ for flushing in the sieving process, enhancing the sieving effect, temporarily storing the slurry passing through the screen in heat insulation equipment, and calculating the volume of the slurry to be V 1
(2) Adding the slurry obtained in the step (1) through a screen into a first-stage filter bag, and centrifuging at a high speed of 1500-2000 r/min to remove particles and filtrate with particle diameters smaller than 22 mu m, wherein hot water with the temperature of 70-80 ℃ is added in batches during the process, and the total amount of the added hot water is 8-10V 1 Centrifuging twice, wherein the adding amount of hot water is 4-5V each time 1 The method comprises the steps of carrying out a first treatment on the surface of the After the first centrifugation, mashing and washing the solid wet material, adding hot water again for high-speed centrifugation for 30-40 min, and carrying out the next step after no filtrate flows out;
(3) Collecting the particles retained in the first-stage filter bag in the step (2), and fully drying to obtain first-stage micron-sized particles with volume average particle size of 25-32 mu m;
(4) Collecting the slurry passing through the first-stage filter bag in the step (2), and then passing through a second-stage electric vibration screen to remove large-size particles with the particle size larger than 15 mu m, wherein the slurry passing through the screen is temporarily stored in heat-insulating equipment, and the volume of the slurry is calculated to be V 2
(5) Adding the slurry obtained in the step (4) into a second-stage filter bag, and performing high-speed centrifugation at 1500-2000 r/min to remove particles with the particle size smaller than 8 mu mAdding 70-80 ℃ hot water into the granules and the filtrate in batches during the period, wherein the total amount of the added hot water is 2-4V 2 Centrifuging twice, wherein the hot water added each time is 1-2V 2 The method comprises the steps of carrying out a first treatment on the surface of the After the first centrifugation, mashing and washing the solid wet material, adding hot water again for high-speed centrifugation for 30-40 min, and carrying out the next step after no filtrate flows out;
(6) Collecting the particles retained in the second-stage filter bag in the step (5), and fully drying to obtain second-stage micron-sized particles with volume average particle size of 10-13 μm;
(7) Adding all the slurry in the step (5) into a third-stage filter bag, and performing high-speed centrifugation at 1500-2000 r/min to remove particles and filtrate with particle diameters smaller than 3 mu m, and performing the next step after no filtrate flows out;
(8) And (3) collecting the particles remained in the third-stage filter bag in the step (7), and fully drying to obtain the third-stage micron-sized particles with the volume average particle size of 4-6 mu m.
2. The method for continuously classifying and collecting micron-sized particles according to claim 1, wherein the micron-sized particles are composite toughening particles formed by reacting a polymer, an epoxy resin and a curing agent.
3. The method for continuously classifying and collecting micron-sized particles according to claim 2, wherein the polymer is polyethersulfone, polyurethane, polyamide, polyimide or polycarbonate.
4. The method for continuously classifying and collecting particles of micron order according to claim 1, wherein in the step (1), the first stage electric vibration screen is 316L material, the mesh number is 400 mesh, and the screen pore diameter is 38.5 μm.
5. The method for continuously classifying and collecting particles according to claim 1, wherein in the step (2), the first stage filter bag is made of polypropylene material, the mesh number is 800 mesh, and the mesh diameter of the filter screen is 22 μm.
6. The method for continuously classifying and collecting particles of micron order according to claim 1, wherein in the step (4), the second-stage electric vibration screen is 316L material, the mesh number is 1000 mesh, and the screen pore diameter is 15 μm.
7. The method for continuously classifying and collecting particles according to claim 1, wherein in the step (5), the second stage filter bag is made of polypropylene material, the mesh number is 2000 mesh, and the mesh diameter of the filter screen is 8 μm.
8. The method for continuously classifying and collecting particles according to claim 1, wherein in the step (7), the third stage filter bag is made of polypropylene material, the mesh number is 2800 mesh, and the pore size of the filter screen is 3 μm.
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